Liquid separatory apparatus



June 21, 1966 M MARCUS ETAL 3,257,170

LIQUID SEPARATORY APPARATUS Filed Nov. 9, 1962 ,/VIHHHH-` INVENTORS MARTIN MARCUS SEYMOUR I. KLEINBERG l suspension, accurately in an easy, simple manner.

United States Patent C 3,257,170 LIQUID SEPARATORY APPARATUS Martin Marcns, 623 Walton Ave., Mamaroneck, N.Y., and Seymour I. Kleinberg, 645 W. 239th St., New York, N.Y.

Filed Nov. 9, 1962, Ser. No. 236,502 3 Claims. (Cl. 23-259) This invention relates to apparatus for separating various uids and in particular relates to a funnel for accurately separating immiscible liquids or solutions of a dispersion.

Often it is necessary to separate the various individual liquids or solutions of a dispersion, such as an emulsion or In the chemical and clinical laboratory, it is often desirable to extract a dissolved material from one solvent into another immiscible solvent, such as water and chloroform. Heretofore, in scientific and clinical work a liquid dispersion, such as an emulsion, often had to be placed in a bottle, and then in a centrifuge to separate the liquids into individual layers. The individual liquids were carefully poured into a special decanter open -to the atmosphere with a stopcock for draining the liquids. The accuracy of the separation of the liquids depended to a great extent on the skill and experience of the operator during the pouring and draining operations, aswell as the separating process being slow vand tedious and requiring a large number of separate pieces of apparatus and entailing considerable extra manipulation.

Therefore, it is an object of the present invention to provide a separatory apparatus that can cooperate with a container capable of being centrifuged and separate the individual components of a dispersion in an easy, facile manner.

Another object of the present invention is to provide a funnel type apparatus mountable onto a conventional container which allows quick, accurate separation of the individual various liquid components of a suspension or emulsion with relatively unskilled help. p

Still anotherobject of the present invention is to provide an attachment to cooperate with a container to smoothlyv separate the individual layers of a dispersion in the container which is adjustable, simple and durable in construction, economical to manufacture, operable by relatively unskilled help and quick and easy to use.

A further object is to provide separatory apparatus which can saturate the fluid contained therein with a gas and remove the fluid from a special gaseous atmosphere and introduce the gas as the fluid is being removed, all inY a simple manner.

A still further object of the present invention is to provide separating apparatus which may dry or evaporate the fluid contained therein.

Still another object of the present invention is to provide a funnel to cooperate with a container to adapt A -apparent to'those skilled in the art from the following detailed description taken in connection with the accompanying drawing which illustrates embodiments of the invention in which:

FIGURE 1 is a front elevational view of a separatory apparatus embodying the present invention cooperating with a vessel;

ICC

i of neck 12 but the outer surface of neck 12 may be ground glass instead. l

A separating funnel indicated generally at 16 has a ground glass surface 18 which sealingly mates with ground glass surface 14 of vessel 10 to provide a fluid-tight joint. If the outer surface of neck 12 is ground, then the inner surface 19 of the neck of funnel 16 is ground to sealingly mate with ground glass surface 12. The cooperating surfaces of container 10l and funnel 16 interconnect to form a fluid-tight seal which may be easily assembled and disassembled.

Advantageously, funnel 16 has a tapering portion 20 of reduced cross sectional area or diameter and has a bore 22 which communicates with the interior of container 10 when mounted thereon and the atmosphere.

.Funnel 16 has a tapered valve aperture 24 extending transversely therethorugh intermediate the length thereof and intersecting bore 22 at its smallest cross sectional area. Valve aperture 24 is contained in a housing 25.

Rotatably mounted in valve aperture 24 is a tapered valve plug 26. Plug 26 is held in seated engagement with aper- -ture 24 by any suitable means. One type, as shown, has the smaller end of plug `26 threaded at 28. Suitable washer 30 and seal means 32 are interposed between the valve housing 25 and a nut 34 threaded onto the threaded portion 28 of plug 26.

Plug 26 is provided at its larger end with a handle 35 for turning and intermediate of its length with a transverse aperture 36 which registers with bore 22 when plug 26 is rotated into position 4as shown in FIGURE 2. When plug 26 is in the rotational position shown in FIGURE 2,

aperture 36 provides a continuation of bore 22 through rupted by valve plug 26.

Valve housing 25 extends transversal beyond bore 22.

Mounted on the extension of valve housing 25 is a tube.

40. Tube 4()` is curved and passes through the tapered portion of funnel |16 and axially through bore 22 in a direction away from plug 26. Tube 40 has a portion 42 extending beyond the end of the ground glass surface to end adjacent the bottom of container 10l when funnel 16 is mounted therein. When the apparatus is in the position shown in FIGURE 2, the end of tube 42 adjacent to the bottom of the container 10 shall extend above the surface of the fluid in the apparatus. tending therethrough.

The smaller end 28 of plug 26 has anI axial bore 46 extending inwardly from the end to preferably intersecting the plane containing the axis of bore 44 of tube 40. Plug 26 has a transverse aperture 48 parallel to aperture 36 and communicating with bore 46. Aperture 48 registers with bore 44 when plug 26 is rotated into position so that bore 22 and aperture 36 are in register. Alternately, aperture 48 does not register with bore 44 when plug 26 is lrotated through an angle of In using the separatory apparatus, vessel 10 contains at least two immiscible liquids indicated at 50 and 52V respectively. As an example, `an aqueous solution and chloroform are added to vessel 1 0. Vessel 10 is sealed by any suitable means such as a cap or plug, not shown, or plug 26 being rotated out of register with bores 22 and 44. The vessel is shaken by suitable means for a short period of time to allow the solute of the aqueous solu- Patented June 2l, 1966 Tube 40 has a bore 44 extion to be extracted by the chloroform. If Ian emulsion lis formed, the vessel may be centrifuged. If centrifugation is necessary, preferably the cap tor plug, not shown, should be used to seal vessel during theJ centrifufging process. After centrifugation, the liquids form two layers, as shown in FIGURES l and 2, with the heavier fluid settling at the bottom. Funnel 16 is mounted on container lil lwith tube 42 extending into container 10. Plug 26 is rotated so that both bores 22 4and 44 are not in register, and container 10 is inverted carefully to avoid remixing the layers of uids 50 and 52. Plug 26 is rotated by means of handle 35 to a position where both bores 22 and 44 are open and extend 4continuously through plug 26. As shown in FIGURE 2, fluid 52 flows from container 10 through bore 22 and aperture 36 and and is collected in any desired manner. Simultaneously, air from the atmosphere Will flow through bore 46 and upwardly through aperture 48 and bore 44 into container 1i) to replace fluid 52 flowing from vessel 10. When the end of iluid 52 passes through the small cross sectional portion 2i of lfunnel 16, plug 26 is rotated to close bores 22 and 44. Since the cross sectional area is small and contiguous to plug 26, great accuracy in isolating the fluids can be obtained.

Fluid Si? is removed from container 10 in the same manner as described above, or funnel 16 is removed and fluid 50 may be poured therefrom.

If an atmosphere other than air is desired in container 10, a source of the desired gas is attached to end 28 of plug 26 and introduced via bore 46. The air is removed through bore 22, which is closed by rotating plug 26 when the desired concentration is reached.

With the present invention1 the interior of container 10 may have its pressure reduced below atmospheric pressure to hasten removal of the liuid or maintain the contents under vacuum. T o accomplish this, the apparatus is placed in its upright position, as shown in FIGURE 1, and handle 35 rotated to close Ibore `44 and have bore 22 open. A vacuum source, not shown, is attached to bore 22 which quickly reduces the pressure within container 1t) to the desired reading. Advantageously, heat or cold is applied to container 10 to hasten removal of the fluid.

With the present invention, the uid may be saturated with gas. Container 10 and funnel 16 are in their upright position, FIGURE l, and bores 22 and 44 are open. A source of the desired gas at a higher pressure than the container is attached to end 28 of plug 26 and the gas introduced into container 10 via bore 44 and bubbles through the Huid.

Another embodiment is shown in FIGURE 3. Funnel 60 has ground surfaces 62 for sealingly cooperating lwith a container having a neck 61. A plug 64 is rotatably mounted transversely to bore 66 and contains an aperture 68. Air tube 70 having a bore 72 interconnects 'a ground surface 62. Neckv 61 has a transverse aperture 74 therethrough communicating with the atmosphere and aligned with bore 72 when funnel 60 is mounted thereon. Bore 72 and aperture 74 register when `funnel 60 is in a certain rotational position to allow air to be introduced into the container as the uid is removed.

While the present invention was indicated as being made of glass, it may be made of plastic or other type of materials chemically resistant to the materials being handled.

The present invention allows a tight seal to be maintained when the desired material is obtained so that the material may be kept under pressure, gas, vacuum for long periods of time.

The invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The construction shown in the drawing and described above is to be considered illustrative only and not restrictive, the scope of the invention being defined by the claims appended hereto.

What is claimed is:

1. Liquid separatory apparatus for `analytical purposes comprising la container having a neck at one end with a smaller cross-sectional area than said container, a funnel detachably and telescopically secured at one end to said container neck and having a generally longitudinally extending bore therein tapering inwardly and away from said container, said bore being small in cross section relative to Ithe cross section of said container, and communieating at one end with the interior of said container, a tube having a bore extending from within said funnel bore to a location within and adjacent the other end of said container, said funnel having -a transversely extending valve bore intersecting said funnel bore at said funnel bores smallest cross sectional area, so that separating liquids c-ontained within said container is accurately controlled, said funnel longitudinally extending away from said container a substantial distance |beyond said valve bore, a manually rotatable plug disposed in said valve bore and having a first aperture extending transversely therethrough for coinciding with said longitudinally extending funnel bore when said plug is in -a predetermined rotational position relative -to said funnel, said tube bore communicating ywith said valve bore, said plug having a second aperture extending partially therethrough and spaced from and parallel to said lirst aperture Iand an axial bore communicating with the atmosphere and said second aperture, said axial bore communicating with the atmosphere remote from said outflow from said funnel bore, so that said plug when in said predetermined rotational position is operable to open said funnel bore and to open a passage from the interior of said container via said tube to the atmosphere without creating turbulence of the liquids contained within said container.

. '2. A separatory funnel for ltelescopically mounting on a neck of a container for separating layers of immiscible liquids for analytical purposes, said funnel having a generally longitudinally extending bore therein tapering inwardly and -away from said container, said bore being small in cross section relative to the cross section of said container and adapted to communicate at one end with the interior of said container, a tube having a bore extending from within said funnel bore to a location within and adjacent the other end of said container when said funnel is operably mounted on said container, said funnel having `a transversely extending valve bore intersecting said funnel bore at said funnel bores smallest cross sectional area so that .separating liquids contained within said container is accurately controlled, said funnel longitudinally extending away from said container a substantial distance beyond said valve bore, a manually rotatable plug disposed in said valve bore and having -a first aperture extending transversely therethrough for coinciding with said longitudinally extending funnel bore when said plug is in a predetermined rotational position relative to said funnel, said tube bore communicating with said valve bore, said plug having a second aperture extending partially therethrough Iand spaced from and parallel to said iirst aperture and an axial bore cornmunicating with the atmosphere and said second aperture, said axial bore communicating with the atmosphere remote from said `outflow from said funnel bore, so that said plug when in said predetermined rotational position is operable to open said funnel bore and to open a passage from the interior of said container via said tube to the atmosphere without creating turbulence of the liquids contained Within said container.

3. A separatory funnel in accordance with claim 2, wherein said plug surrounding said axial bore communieating with the atmosphere is threaded and adapted to communicate with a source lof inert gas.

(References on following page) References Cited bythe Examiner UNITED FOREIGN PATENTS STATES PATENTS 530,102 2/1923 Fra-nca. Cooper 3 26 1,011,582 7/1957 Germany.

'111 h 222-4 4 grtt l 23 2g2 5 REUBEN FRIEDMAN, Pnjmmy Examiner. H ustinx 23-292 H. B. THORNTON, Examiner. fsrlglffu-:jl s. ZAHARNA, Assistant Examiner; 

1. LIQUID SEPARATORY APPARATUS FOR ANALYTICAL PURPOSES COMPRISING A CONTAINER HAVING A NECK AT ONE END WITH A SMALLER CROSS-SECTIONAL AREA THAN SAID CONTAINER, A FUNNEL DETACHABLY AND TELESCOPICALLY SECURED AT ONE END TO SAID CONTAINER NECK AND HAVING A GENERALLY LONGITUDINALLY EXTENDING BORE THEREIN TAPERING INWARDLY AND AWAY FROM SAID CONTAINER, SAID BORE BEING SMALL IN CROSS SECTION RELATIVE TO THE CROSS SECTION OF SAID CONTAINER, AND COMMUNICATING AT ONE END WITH THE INTERIOR OF SAID CONTAINER, A TUBE HAVING A BORE EXTENDING FROM WITHIN SAID FUNNEL BORE TO A LOCATION WITHIN AND ADJACENT THE OTHER END OF SAID CONTAINER, SAID FUNNEL HAVING A TRANSVERSELY EXTENDING VALVE BORE INTERSECTING SAID FUNNEL BORE AT SAID FUNNEL BORE''S SMALLEST CROSS SECTIONAL AREA, SO THAT SEPARATING LIQUIDS CONTAINED WITHIN SAID CONTAINER IS ACCURATELY CONTROLLED, SAID FUNNEL LONGITUDINALLY EXTENDING AWAY FROM SAID CONTAINER A SUBSTANTIAL DISTANCE BEYOND SAID VALVE BORE, A MANUALLY ROTATABLE PLUG DISPOSED IN SAID VALVE BORE AND HAVING A FIRST APERTURE EXTENDING TRANSVERSELY THERETHROUGH FOR COINCIDING WITH SAID LONGITUDINALLY EXTENDING FUNNEL BORE WHEN SAID PLUG IS IN A PREDETERMINED ROTATIONAL POSITION RELATIVE TO SAID FUNNEL, SAID TUBE BORE COMMUNICATING WITH SAID VALVE BORE, SAID PLUG HAVING A SECOND APERTURE EXTENDING PARTIALLY THERETHROUGH AND SPACED FROM AND PARALLEL TO SAID FIRST APERTURE AND AN AXIAL BORE COMMUNICATING WITH THE ATMOSPHERE AND SAID SECOND APERTURE, SAID AXIAL BORE COMMUNICATING WITH THE ATMOSPHERE REMOTE FROM SAID OUTFLOW FROM SAID FUNNEL BORE, SO THAT SAID PLUG WHEN IN SAID PREDETERMINED ROTATIONAL POSITION IS OPERABLE TO OPEN SAID FUNNEL BORE AND TO OPEN A PASSAGE FROM THE INTERIOR OF SAID CONTAINER VIA SAID TUBE TO THE ATMOSPHERE WITHOUT CREATING TURBULENCE OF THE LIQUIDS CONTAINED WITHIN SAID CONTAINER. 